CN105506739A - Process for manufacturing sapphire crystal rod from sapphire pieces - Google Patents
Process for manufacturing sapphire crystal rod from sapphire pieces Download PDFInfo
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- CN105506739A CN105506739A CN201510748328.6A CN201510748328A CN105506739A CN 105506739 A CN105506739 A CN 105506739A CN 201510748328 A CN201510748328 A CN 201510748328A CN 105506739 A CN105506739 A CN 105506739A
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- sapphire
- fragment
- speed
- tungsten crucible
- heating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/20—Aluminium oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B17/00—Single-crystal growth onto a seed which remains in the melt during growth, e.g. Nacken-Kyropoulos method
Abstract
The present invention relates to the technical field of crystal material processing, and discloses a process for manufacturing sapphire crystal rod from sapphire pieces, and the process comprises the following steps: seed crystal selection, to be more specific, taking a certain weight of sapphire pieces for heating in a 500 DEG C-800 DEG C vacuum heating furnace for 1-2h, taking the sapphire pieces out after cooling, picking out seed crystals without crystal boundaries from the sapphire pieces, and loading the picked seed crystals onto a seed crystal holder in a kyropoulos furnace; processing and loading of the sapphire pieces in the furnace; seeding, to be more specific, vacuumizing the kyropoulos furnace, first heating with a heater, thermally insulating for 0.5-1h, secondarily heating with the heater until the temperature in the furnace is raised by 20 DEG C-40 DEG C, thermally insulating for 0.5-1h, reducing the heater power, after the temperature in the furnace is reduced by 20 DEG C-40 DEG C, thermally insulating for 1-2h, rotating to drop the seed crystal holder for contact and seeding; and shoulder expansion growth, equal diameter growth, and the like after the seeding. The process has the beneficial effects of more stable and reliable seeding, less sapphire internal crystal boundaries, and high quality.
Description
Technical field
The present invention relates to crystalline material processing and manufacturing technical field, particularly relate to a kind of technique utilizing sapphire fragment to manufacture sapphire ingot.
Background technology
Sapphire has excellent physics, machinery, chemistry and infrared light transmission performance, is the material that the fields such as microelectronics, aerospace, military project are badly in need of always.Adopt at present usually kyropoulos to manufacture sapphire ingot, highly purified aluminium sesquioxide Mi Dui in crucible and heat fused, then rotated by seed crystal and carry out seeding, expand shoulder, finally make sapphire ingot.Sapphire ingot can produce the widely different fragment of a lot of granular size in following process process, and these sapphire fragments also can direct marketing usually, but selling price is lower, and utilization ratio is lower; In order to improve value and the utilization ratio of sapphire fragment, some producer using sapphire fragment as raw material, sapphire is made with kyropoulos again after newly melting down, but the sapphire ingot finally made is larger with the quality gap of the sapphire ingot directly adopting high purity raw material to make, because the lattice arrangements in sapphire fragment is different from the lattice arrangements in aluminium sesquioxide starting material, if after therefore adopting common kyropoulos technique that sapphire crystal is made in the fusing of sapphire fragment, it can't meet the quality requirement.
Summary of the invention
The present invention is in order to after solving direct employing kyropoulos technique of the prior art sapphire fragment being made sapphire ingot, the ropy deficiency of sapphire ingot, provide the technique that a kind of sapphire fragment manufactures sapphire ingot, few by the inner crystal boundary of the sapphire ingot of this manufacture technics, total quality is more even.
To achieve these goals, the present invention adopts following technical scheme:
Utilize sapphire fragment to manufacture a technique for sapphire ingot, comprise the following steps:
A, seed crystal are selected: the sapphire fragment getting certainweight, 1-2h is heated in the vacuum furnace of 500 DEG C-800 DEG C, take out after cooling, in sapphire fragment, pick out the seed crystal not having crystal boundary, the seed crystal at the place of selecting is installed on the seedholder in the raw stove of bubble;
B, the process of sapphire fragment, shove charge: with washed with de-ionized water sapphire fragment, after cleaning, quenching is pulverized and is formed Particle Phase to uniform sapphire particle, then use washed with de-ionized water sapphire particle, sapphire particle is loaded tungsten crucible, tungsten crucible is placed in the raw stove of bubble;
C, seeding: vacuumize in the raw stove of bubble, well heater once heats, and is heated to sapphire particle and melts formation melt completely, insulation 0.5-1h; Well heater second-heating, is heated to in-furnace temperature and raises 20 DEG C-40 DEG C, insulation 0.5-1h; Reduce heater power, in-furnace temperature is incubated 1-2h after reducing by 20 DEG C-40 DEG C, and seedholder rotates and declines, seed crystal lower end and melt contacts, seeding;
D, seeding terminate the growth of rear expansion shoulder, isodiametric growth;
After e, crystal bar grow up to completely, reduce heater power, be cooled to room temperature with the speed of 20-30 DEG C/h, obtain sapphire ingot.
Seed crystal is directly picked out from sapphire particle, thus ensures that seed crystal internal crystal structure is more consistent with the crystalline structure in melt, and in seeding process, seed crystal can fast and Melt Stability structure, and seeding is stablized more, reliably; Lattice distribution in different sapphire particle there are differences, and after well heater heat fused, bath composition is uneven, pass through second-heating, lattice is evenly distributed, consistence is high, thus ensure the sapphire ingot steady quality made, each site component consistence of sapphire ingot is good; Second-heating can also make the gas overflowing of melt internal residual.
As preferably, in step c, in well heater heat-processed, tungsten crucible rotates with the speed of 5-10rpm, and in the insulating process after the first heating, tungsten crucible rotates with the speed of 1-2rpm.In heat-processed, tungsten crucible rotates, and plays a stirring action, and make melt more even, slow down in insulating process rotating speed, and after insulation, melt reaches once balance state.
As preferably, the sense of rotation of tungsten crucible in a heat-processed with once heat after sense of rotation in insulating process contrary.Twice sense of rotation is contrary, melt is distributed more even.
As preferably, in step c, in well heater post bake process, tungsten crucible rotates with the speed of 2-4rpm, and in the insulating process after second-heating, tungsten crucible rotates with the speed of 0.5-1rpm, and after second-heating, insulation terminate, tungsten crucible stops operating.
As preferably, the expansion shoulder growth phase in steps d, reduce heater power, with the cooling of the speed of 0.5-2 DEG C/h, seedholder is so that the speed of 0.25mm-0.35mm/h to be moved.Because melt crystallization is an exothermic process, along with the increase of external diameter, melt heat release also increases, and therefore needs slowly to reduce heater power to keep expanding in shoulder growth, and the growth temperature of sapphire at different diameter place close to consistent, thus improves sapphire quality.
As preferably, in the isodiametric growth stage in steps d, reduce heater power, with the cooling of the speed of 1-2.5 DEG C/h, seedholder is so that the speed of 0.15mm-0.25mm/h to be moved.
Therefore, the present invention has following beneficial effect: (1) seed crystal is directly picked out from sapphire particle, thus ensures that seed crystal internal crystal structure is more consistent with the crystalline structure in melt, in seeding process, seed crystal can be combined with Melt Stability fast, and seeding is more stable, reliable; (2) processed melt by twice rotary heating, the mode of once lowering the temperature, the lattice in melt is distributed and is tending towards even, the inner crystal boundary of the sapphire made is few, quality is high.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1: a kind of technique utilizing sapphire fragment to manufacture sapphire ingot, comprises the following steps:
A, seed crystal are selected: the sapphire fragment getting certainweight, in the vacuum furnace of 500 DEG C, heat 2h, take out, pick out the seed crystal not having crystal boundary in sapphire fragment after cooling, are installed to by the seed crystal at the place of selecting on the seedholder in the raw stove of bubble;
B, the process of sapphire fragment, shove charge: with washed with de-ionized water sapphire fragment, after cleaning, quenching is pulverized and is formed Particle Phase to uniform sapphire particle, then use washed with de-ionized water sapphire particle, sapphire particle is loaded tungsten crucible, tungsten crucible is placed in the raw stove of bubble;
C, seeding: vacuumize in the raw stove of bubble, well heater once heats, in heat-processed, tungsten crucible rotates with the speed of 5rpm, be heated to sapphire particle and melt formation melt completely, insulation 0.5h, in insulating process, tungsten crucible rotates with the speed of 1rpm, and the sense of rotation of tungsten crucible is contrary with the sense of rotation in a heat-processed; Well heater second-heating, tungsten crucible rotates with the speed of 2rpm, be heated to in-furnace temperature and raise 20 DEG C, insulation 0.5h, in insulating process, tungsten crucible rotates with the speed of 0.5rpm, and in second-heating, insulating process, the sense of rotation of tungsten crucible is identical with the sense of rotation once heated in rear insulating process, after second-heating, insulation terminate, tungsten crucible stops operating; Reduce heater power, in-furnace temperature is incubated 1h after reducing by 20 DEG C, and seedholder rotates and declines, seed crystal lower end and melt contacts, seeding;
D, the growth of expansion shoulder, expand shoulder growth phase, reduction heater power, with the cooling of the speed of 0.5 DEG C/h, seedholder is so that the speed of 0.25mm/h to be moved; Isodiametric growth, reduces heater power, and with the cooling of the speed of 1 DEG C/h, seedholder is so that the speed of 0.15mm/h to be moved;
After e, crystal bar grow up to completely, reduce heater power, be cooled to room temperature with the speed of 20 DEG C/h, obtain sapphire ingot.
Embodiment 2: a kind of technique utilizing sapphire fragment to manufacture sapphire ingot, comprises the following steps:
A, seed crystal are selected: the sapphire fragment getting certainweight, in the vacuum furnace of 650 DEG C, heat 1.5h, take out, pick out the seed crystal not having crystal boundary in sapphire fragment after cooling, are installed to by the seed crystal at the place of selecting on the seedholder in the raw stove of bubble;
B, the process of sapphire fragment, shove charge: with washed with de-ionized water sapphire fragment, after cleaning, quenching is pulverized and is formed Particle Phase to uniform sapphire particle, then use washed with de-ionized water sapphire particle, sapphire particle is loaded tungsten crucible, tungsten crucible is placed in the raw stove of bubble;
C, seeding: vacuumize in the raw stove of bubble, well heater once heats, in heat-processed, tungsten crucible rotates with the speed of 8rpm, be heated to sapphire particle and melt formation melt completely, insulation 0.8h, in insulating process, tungsten crucible rotates with the speed of 1.5rpm, and the sense of rotation of tungsten crucible is contrary with the sense of rotation in a heat-processed; Well heater second-heating, tungsten crucible rotates with the speed of 3rpm, be heated to in-furnace temperature and raise 30 DEG C, insulation 0.8h, in insulating process, tungsten crucible rotates with the speed of 0.8rpm, and in second-heating, insulating process, the sense of rotation of tungsten crucible is identical with the sense of rotation once heated in rear insulating process, after second-heating, insulation terminate, tungsten crucible stops operating; Reduce heater power, in-furnace temperature is incubated 1.5h after reducing by 30 DEG C, and seedholder rotates and declines, seed crystal lower end and melt contacts, seeding;
D, the growth of expansion shoulder, expand shoulder growth phase, reduction heater power, with the cooling of the speed of 1.5 DEG C/h, seedholder is so that the speed of 0.3mm/h to be moved; Isodiametric growth, reduces heater power, and with the cooling of the speed of 2 DEG C/h, seedholder is so that the speed of 0.2mm/h to be moved;
After e, crystal bar grow up to completely, reduce heater power, be cooled to room temperature with the speed of 25 DEG C/h, obtain sapphire ingot.
Embodiment 3: a kind of technique utilizing sapphire fragment to manufacture sapphire ingot, comprises the following steps:
A, seed crystal are selected: the sapphire fragment getting certainweight, in the vacuum furnace of 800 DEG C, heat 1h, take out, pick out the seed crystal not having crystal boundary in sapphire fragment after cooling, are installed to by the seed crystal at the place of selecting on the seedholder in the raw stove of bubble;
B, the process of sapphire fragment, shove charge: with washed with de-ionized water sapphire fragment, after cleaning, quenching is pulverized and is formed Particle Phase to uniform sapphire particle, then use washed with de-ionized water sapphire particle, sapphire particle is loaded tungsten crucible, tungsten crucible is placed in the raw stove of bubble;
C, seeding: vacuumize in the raw stove of bubble, well heater once heats, in heat-processed, tungsten crucible rotates with the speed of 10rpm, be heated to sapphire particle and melt formation melt completely, insulation 1h, in insulating process, tungsten crucible rotates with the speed of 2rpm, and the sense of rotation of tungsten crucible is contrary with the sense of rotation in a heat-processed; Well heater second-heating, tungsten crucible rotates with the speed of 2rpm, be heated to in-furnace temperature and raise 40 DEG C, insulation 1h, in insulating process, tungsten crucible rotates with the speed of 1rpm, and in second-heating, insulating process, the sense of rotation of tungsten crucible is identical with the sense of rotation once heated in rear insulating process, after second-heating, insulation terminate, tungsten crucible stops operating; Reduce heater power, in-furnace temperature is incubated 2h after reducing by 40 DEG C, and seedholder declines, seed crystal lower end and melt contacts, seeding;
D, the growth of expansion shoulder, expand shoulder growth phase, reduction heater power, with the cooling of the speed of 2 DEG C/h, seedholder is so that the speed of 0.35mm/h to be moved; Isodiametric growth, reduces heater power, and with the cooling of the speed of 2.5 DEG C/h, seedholder is so that the speed of 0.25mm/h to be moved;
After e, crystal bar grow up to completely, reduce heater power, be cooled to room temperature with the speed of 30 DEG C/h, obtain sapphire ingot.
Claims (6)
1. utilize sapphire fragment to manufacture a technique for sapphire ingot, it is characterized in that, comprise the following steps:
A, seed crystal are selected: the sapphire fragment getting certainweight, 1-2h is heated in the vacuum furnace of 500 DEG C-800 DEG C, take out after cooling, in sapphire fragment, pick out the seed crystal not having crystal boundary, the seed crystal at the place of selecting is installed on the seedholder in the raw stove of bubble;
B, the process of sapphire fragment, shove charge: with washed with de-ionized water sapphire fragment, after cleaning, quenching is pulverized and is formed Particle Phase to uniform sapphire particle, then use washed with de-ionized water sapphire particle, sapphire particle is loaded tungsten crucible, tungsten crucible is placed in the raw stove of bubble;
C, seeding: vacuumize in the raw stove of bubble, well heater once heats, and is heated to sapphire particle and melts formation melt completely, insulation 0.5-1h; Well heater second-heating, is heated to in-furnace temperature and raises 20 DEG C-40 DEG C, insulation 0.5-1h; Reduce heater power, in-furnace temperature is incubated 1-2h after reducing by 20 DEG C-40 DEG C, and seedholder rotates and declines, seed crystal lower end and melt contacts, seeding;
D, seeding terminate the growth of rear expansion shoulder, isodiametric growth;
After e, crystal bar grow up to completely, reduce heater power, be cooled to room temperature with the speed of 20-30 DEG C/h, obtain sapphire ingot.
2. a kind of technique utilizing sapphire fragment to manufacture sapphire ingot according to claim 1, is characterized in that, in step c, in well heater heat-processed, tungsten crucible rotates with the speed of 5-10rpm, and in the insulating process after the first heating, tungsten crucible rotates with the speed of 1-2rpm.
3. a kind of technique utilizing sapphire fragment to manufacture sapphire ingot according to claim 2, it is characterized in that, the sense of rotation of tungsten crucible in a heat-processed is contrary with the sense of rotation once heated in rear insulating process.
4. a kind of technique utilizing sapphire fragment to manufacture sapphire ingot according to claim 1 and 2, it is characterized in that, in step c, in well heater post bake process, tungsten crucible rotates with the speed of 2-4rpm, and in the insulating process after second-heating, tungsten crucible rotates with the speed of 0.5-1rpm, after second-heating, insulation terminate, tungsten crucible stops operating.
5. a kind of technique utilizing sapphire fragment to manufacture sapphire ingot according to claim 1, it is characterized in that, the expansion shoulder growth phase in steps d, reduces heater power, with the cooling of the speed of 0.5-2 DEG C/h, seedholder is so that the speed of 0.25mm-0.35mm/h to be moved.
6. a kind of technique utilizing sapphire fragment to manufacture sapphire ingot according to claim 1 or 2 or 3 or 5, it is characterized in that, the isodiametric growth stage in steps d, reduce heater power, with the cooling of the speed of 1-2.5 DEG C/h, seedholder is so that the speed of 0.15mm-0.25mm/h to be moved.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009120453A (en) * | 2007-11-16 | 2009-06-04 | Sumitomo Metal Mining Co Ltd | Method of manufacturing aluminum oxide single crystal |
| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN103074671A (en) * | 2012-11-05 | 2013-05-01 | 浙江东海蓝玉光电科技有限公司 | Soaking method for reducing large size sapphire crystal bubble |
| CN104562198A (en) * | 2014-12-12 | 2015-04-29 | 宁波循泽电子科技有限公司 | Method for improving growth of kyropoulos method sapphire single crystal |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN104674339A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Method for reducing crystal boundary in process of growing large sapphire by virtue of kyropoulos method |
| CN104674340A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Rotary necking and seeding control method used in large-size sapphire crystal growth through kyropoulos method |
| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
-
2015
- 2015-11-06 CN CN201510748328.6A patent/CN105506739A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009120453A (en) * | 2007-11-16 | 2009-06-04 | Sumitomo Metal Mining Co Ltd | Method of manufacturing aluminum oxide single crystal |
| CN103074671A (en) * | 2012-11-05 | 2013-05-01 | 浙江东海蓝玉光电科技有限公司 | Soaking method for reducing large size sapphire crystal bubble |
| CN102943303A (en) * | 2012-11-14 | 2013-02-27 | 上海施科特光电材料有限公司 | Method to restrain bubbles in process of growing sapphire by using kyropoulos method |
| CN104562198A (en) * | 2014-12-12 | 2015-04-29 | 宁波循泽电子科技有限公司 | Method for improving growth of kyropoulos method sapphire single crystal |
| CN104674345A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Seeding control method for large-size sapphire crystals growing through Kyropulos method |
| CN104674339A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Method for reducing crystal boundary in process of growing large sapphire by virtue of kyropoulos method |
| CN104674340A (en) * | 2014-12-26 | 2015-06-03 | 浙江东海蓝玉光电科技有限公司 | Rotary necking and seeding control method used in large-size sapphire crystal growth through kyropoulos method |
| CN104695010A (en) * | 2014-12-26 | 2015-06-10 | 浙江东海蓝玉光电科技有限公司 | Improved Kyropulos method for quickly preparing large-size sapphire crystals |
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